HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethyl Acetate → HCID 69019837, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Bromoacetyl bromide | HCID 61147 | — |
| Reactant | HCID 22714353 | HCID 22714353 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Product | HCID 69019837 | HCID 69019837 | 93% |
Reaction Steps
Bromo-acetyl bromide (0.0138 mol) was added slowly at 5° C. to a mixture of (±)-[2-amino-5-[(4-chlorophenyl)hydroxy(1-methyl-1H-imidazol-5-yl)methyl]phenyl](3-chlorophenyl)methanone (prepared as described in WO 97/21701) (0.0137 mol) in acetic acid (60 ml). The mixture was stirred for 15 min and poured out into EtOAc and NaOH 0.5N. The organic layer was separated, washed with water, dried (MgSO4), filtered and the solvent was evaporated till dryness, yielding 7.3 g (93%) of 2-bromo-N-[2-(3-chlorobenzoyl)-4-[(4-chlorophenyl)hydroxy(1-methyl-1H-imidazol-5-yl)methyl]phenyl]-acetamide (intermediate 4).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07153958B2 |
| Source dataset | uspto-grants-2006_12 |
| ORD ID | ord-056b55f2913f4c82a2a3111791c7234d |
| Source note | uspto-grants-2006_12 |